関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 3-Chloro-1-butene | HCID 11242 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | tert-Butyl 4-hydroxybenzoate | HCID 117640 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 3-[4-(tert-Butoxycarbonyl)phenoxy]-1-butene | HCID 85815385 | 60.2% |
反応手順
A solution of 1,1-dimethylethyl 4-hydroxybenzoate (5.0 g, 25.7 mmol) in N,N-dimethylformamide (35 ml) was treated with a solution of sodium hydroxide (1.14 g, 35.1 mmol) in water (2 mL). Then 3-chloro-1-butene (3.06 g, 33.8 mmol) was added and the resulting mixture was heated at 45° C. for 5 hours. The cooled mixture was diluted with toluene, washed with water, dried (magnesium sulfate) and concentrated under reduced pressure. Chromatography of the residue on silica gel (elution toluene-hexane, 1:1) gave 3.84 g (60%) of the title material as a clear oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06924391B2 |
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| 出典データセット | uspto-grants-2005_08 |
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| ORD ID | ord-73c47ae0e65848279697a28c9936002c |
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| 出典メモ | uspto-grants-2005_08 |
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